CN112251002A - PBS (Poly Butylene succinate) degradable packaging material with excellent toughness and temperature resistance and preparation method thereof - Google Patents
PBS (Poly Butylene succinate) degradable packaging material with excellent toughness and temperature resistance and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/326—Magnesium phosphate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
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- C08K2003/328—Phosphates of heavy metals
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- C08L2201/06—Biodegradable
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention relates to the technical field of packaging materials, in particular to a PBS (Poly Butylene succinate) degradable packaging material with excellent toughness and temperature resistance and a preparation method thereof. The product prepared by using the PBS with low price has excellent toughness and temperature resistance, can be completely biodegraded, is a good substitute of the existing non-degradable packaging bag, and has the advantages of simple preparation method, easy implementation of production process, environmental protection and saving.
Description
Technical Field
The invention relates to the technical field of packaging materials, in particular to a PBS (Poly Butylene succinate) degradable packaging material with excellent toughness and temperature resistance and a preparation method thereof.
Background
At present, other biodegradable plastics such as polylactic acid, polyhydroxyalkanoate, polycaprolactone and the like are expensive, lack of good heat resistance and mechanical properties, low in heat deformation temperature, and single in processing method, and special process equipment is needed for production, so that long-term application and development of the biodegradable plastics are not facilitated.
The poly (butylene succinate) can be applied to the field of national civilization such as packaging materials, disposable environment-friendly products, agricultural and forestry products, medical materials and the like. PBS belongs to thermoplastic resin, has good processing performance, can be molded on common processing molding equipment, and can be processed by molding methods such as injection molding, blow molding, film blowing, plastic sucking, laminating, foaming, spinning and the like. PBS is a polymer with good biodegradability, compared with biodegradable plastics such as polylactic acid, polyhydroxyalkanoate, polycaprolactone and the like, PBS has relatively low price, excellent mechanical property and good heat resistance, and is a key point in the research and development of biodegradable plastics at home and abroad.
Disclosure of Invention
The invention provides a PBS (Poly Butylene succinate) degradable packaging material with excellent toughness and temperature resistance and a preparation method thereof, overcomes the defects of the prior art, and can effectively solve the problems of high price, poor heat resistance and mechanical properties and low thermal deformation temperature of the existing biodegradable material.
One of the technical schemes of the invention is realized by the following measures: the PBS degradation packaging material with excellent toughness and temperature resistance comprises, by weight, 30-70 parts of PBS, 10-40 parts of PBST, 10-30 parts of PBAT, 2-7 parts of a compatilizer, 0.3-1.5 parts of a nucleating agent, 0.3-1.5 parts of a heat-resistant agent, 1-3 parts of a plasticizer and 1-30 parts of an inorganic filler, and is prepared by the following method: firstly, uniformly mixing required amounts of PBS, PBST, PBAT, compatilizer, nucleating agent, heat-resistant agent, plasticizer and inorganic filler to obtain a primary mixture; secondly, granulating the primary mixture at 75-190 ℃ to obtain granular mixed resin; and thirdly, blowing the particle mixed resin into a film with smooth and non-frosted surface under the conditions of 130-190 ℃ and 200-360 r/min of rotation speed to obtain the PBS degradable packaging material with excellent toughness and temperature resistance.
The following is a further optimization or/and improvement of one of the above-mentioned technical solutions of the invention:
the raw materials comprise, by weight, 55-60 parts of PBS, 10-14 parts of PBST, 10-14 parts of PBAT, 3 parts of a compatilizer, 0.5-1 part of a nucleating agent, 1 part of a heat-resistant agent, 1-2 parts of a plasticizer and 10-20 parts of an inorganic filler.
The compatilizer is more than one of tetrabutyl titanate, succinic acid, sebacic acid, basf ADR4370, MDI, TDI and dicumyl peroxide.
The nucleating agent is silicon dioxide, and the mesh number of the silicon dioxide is 3000 meshes to 5000 meshes.
The heat-resistant agent is more than one of zirconium phosphate, magnesium phosphate, calcium stearate, magnesium stearate and barium stearate.
The plasticizer is one or more of phthalate, terephthalate and acetyl tributyl citrate.
The inorganic filler is more than one of calcium carbonate, talcum powder, montmorillonite, mica and magnesium salt whisker.
The second technical scheme of the invention is realized by the following measures: a preparation method of a PBS degradation packaging material with excellent toughness and temperature resistance is carried out according to the following steps: firstly, uniformly mixing required amounts of PBS, PBST, PBAT, compatilizer, nucleating agent, heat-resistant agent, plasticizer and inorganic filler to obtain a primary mixture; secondly, granulating the primary mixture at 75-190 ℃ to obtain granular mixed resin; and thirdly, blowing the particle mixed resin into a film with smooth and non-frosted surface under the conditions of 130-190 ℃ and 200-360 r/min of rotation speed to obtain the PBS degradable packaging material with excellent toughness and temperature resistance.
The following is further optimization or/and improvement of the second technical scheme of the invention:
the compatilizer is more than one of tetrabutyl titanate, succinic acid, sebacic acid, basf ADR4370, MDI, TDI and dicumyl peroxide; or/and the nucleating agent is silicon dioxide, and the mesh number of the silicon dioxide is 3000-5000 meshes; or/and the heat-resistant agent is more than one of zirconium phosphate, magnesium phosphate, calcium stearate, magnesium stearate and barium stearate.
The plasticizer is more than one of phthalate, terephthalate and acetyl tributyl citrate; or/and the inorganic filler is more than one of calcium carbonate, talcum powder, montmorillonite, mica and magnesium salt whisker.
The product prepared by using the PBS with low price has excellent toughness and temperature resistance, can be completely biodegraded, is a good substitute of the existing non-degradable packaging bag, and has the advantages of simple preparation method, easy implementation of production process, environmental protection and saving.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments may be determined according to the technical solutions and practical situations of the present invention. The various chemical reagents and chemical articles mentioned in the invention are all the chemical reagents and chemical articles which are well known and commonly used in the prior art, unless otherwise specified; the percentages in the invention are mass percentages unless otherwise specified; the solution in the present invention is an aqueous solution in which the solvent is water, for example, a hydrochloric acid solution is an aqueous hydrochloric acid solution, unless otherwise specified; the normal temperature and room temperature in the present invention generally mean a temperature of 15 ℃ to 25 ℃, and are generally defined as 25 ℃.
The invention is further described below with reference to the following examples:
example 1: the PBS degradation packaging material with excellent toughness and temperature resistance comprises, by weight, 30-70 parts of PBS, 10-40 parts of PBST, 10-30 parts of PBAT, 2-7 parts of a compatilizer, 0.3-1.5 parts of a nucleating agent, 0.3-1.5 parts of a heat-resistant agent, 1-3 parts of a plasticizer and 1-30 parts of an inorganic filler, and is prepared by the following method: firstly, uniformly mixing required amounts of PBS, PBST, PBAT, compatilizer, nucleating agent, heat-resistant agent, plasticizer and inorganic filler to obtain a primary mixture; secondly, granulating the primary mixture at 75-190 ℃ to obtain granular mixed resin; and thirdly, blowing the particle mixed resin into a film with smooth and non-frosted surface under the conditions of 130-190 ℃ and 200-360 r/min of rotation speed to obtain the PBS degradable packaging material with excellent toughness and temperature resistance.
In the invention, PBS is poly butylene succinate, PBST is poly butylene succinate-co-butylene terephthalate, PBAT is poly adipic acid/butylene terephthalate. The density of the PBS selected by the invention is 1.26g/cm3The melt index was 4g/10min to 15g/10min (detection conditions 190 ℃ C., 2.16 kg). PBST is a completely biodegradable product and can play a toughening role. The density of PBAT can be selected to be 1.15g/cm3To 1.36g/cm3And the weight-average molecular weight is 80000Da to 130000 Da. The invention comprises PBS, PBST, PBAT, compatilizer, nucleating agent and heat resistanceThe agent, plasticizer and inorganic filler are conventionally known and commercially available materials.
Example 2: the PBS degradation packaging material with excellent toughness and temperature resistance comprises, by weight, 30 parts or 70 parts of PBS, 10 parts or 40 parts of PBST, 10 parts or 30 parts of PBAT, 2 parts or 7 parts of a compatilizer, 0.3 part or 1.5 parts of a nucleating agent, 0.3 part or 1.5 parts of a heat-resistant agent, 1 part or 3 parts of a plasticizer and 1 part or 30 parts of an inorganic filler, and is prepared by the following method: firstly, uniformly mixing required amounts of PBS, PBST, PBAT, compatilizer, nucleating agent, heat-resistant agent, plasticizer and inorganic filler to obtain a primary mixture; secondly, granulating the primary mixture at 75 ℃ or 190 ℃ to obtain granular mixed resin; and thirdly, blowing the particle mixed resin into a film with smooth and non-frosted surface under the conditions of 130 ℃ or 190 ℃ and 200r/min or 360r/min of rotating speed to obtain the PBS degradable packaging material with excellent toughness and temperature resistance.
In the prior art, other biodegradable materials such as polylactic acid, polyhydroxyalkanoate, polycaprolactone and the like have the disadvantages of high price, lack of good heat resistance and mechanical properties, low thermal deformation temperature, need of special modified equipment for production, strict processing environment requirements, single processing method and are not beneficial to long-term application and development of biodegradable plastics; the PBS degradable packaging material with excellent toughness and temperature resistance prepared by the invention has low requirements on production equipment, can be subjected to various molding processing on the existing plastic processing general equipment, and can be blended with a large amount of fillers such as calcium carbonate, talcum powder and the like, so that the cost of the PBS material is reduced. The production of the PBS degradable packaging material with excellent toughness and temperature resistance can be directly popularized and processed on the prior common polyolefin processing equipment, is suitable for harsh processing environments such as injection molding, extrusion, plastic suction and the like, can be produced by slightly modifying the prior common polyester production equipment, seriously excesses the productivity of the prior domestic polyester equipment, and provides a new opportunity for the excess polyester equipment by modifying and producing the PBS degradable packaging material with excellent toughness and temperature resistance. Compared with the existing PLA (polylactic acid), the softening point of the PLA is only 58 ℃, the softening point of the PBS can reach 101 ℃, the usable temperature range of the PBS is-30 ℃ to 100 ℃, the PBS can be applied in a boiling water environment, and the application field of the PLA is limited to a certain extent due to the limitation of the softening point. PLA is a typical hydrolysis degradation polymer material, a harsh drying environment is required in the storage process, the material must be packaged by aluminum and plastic, the storage period cannot exceed 2 years, the storage period does not exceed 6 months in non-sealed packaging, and the storage period is only a few hours at 50 ℃. Therefore, the storage cost of PLA articles is high. The PBS degradable packaging material with excellent toughness and temperature resistance is easier to store than PLA products, can be stored for a long time without directly contacting soil and natural water rich in microorganisms in the daily storage process, and can not be degraded.
Example 3: as optimization of the above embodiment, the raw materials include, by weight, 55 to 60 parts of PBS, 10 to 14 parts of PBST, 10 to 14 parts of PBAT, 3 parts of a compatibilizer, 0.5 to 1 part of a nucleating agent, 1 part of a heat-resistant agent, 1 to 2 parts of a plasticizer, and 10 to 20 parts of an inorganic filler.
Example 4: in the optimization of the embodiment, the compatilizer is more than one of tetrabutyl titanate, succinic acid, sebacic acid, basf ADR4370, MDI, TDI and dicumyl peroxide. MDI is diphenylmethane diisocyanate and TDI is toluene diisocyanate.
Example 5: as optimization of the above embodiment, the nucleating agent is silicon dioxide, and the mesh number of the silicon dioxide is 3000 meshes to 5000 meshes.
Example 6: in the optimization of the above embodiment, the heat-resistant agent is one or more of zirconium phosphate, magnesium phosphate, calcium stearate, magnesium stearate, and barium stearate.
Example 7: in the optimization of the embodiment, the plasticizer is more than one of phthalate, terephthalate and acetyl tributyl citrate.
Example 8: as optimization of the above embodiment, the inorganic filler is one or more of calcium carbonate, talc, montmorillonite, mica, and magnesium salt whisker.
Example 9: the preparation method of the PBS degradable packaging material with excellent toughness and temperature resistance is carried out according to the following steps: firstly, uniformly mixing required amounts of PBS, PBST, PBAT, compatilizer, nucleating agent, heat-resistant agent, plasticizer and inorganic filler to obtain a primary mixture; secondly, granulating the primary mixture at 75 ℃ or 190 ℃ to obtain granular mixed resin; and thirdly, blowing the particle mixed resin into a film with smooth and non-frosted surface under the conditions of 130 ℃ or 190 ℃ and 200r/min or 360r/min of rotating speed to obtain the PBS degradable packaging material with excellent toughness and temperature resistance.
Example 10: as optimization of the embodiment, the compatilizer is more than one of tetrabutyl titanate, succinic acid, sebacic acid, basf ADR4370, MDI, TDI and dicumyl peroxide; or/and the nucleating agent is silicon dioxide, and the mesh number of the silicon dioxide is 3000-5000 meshes; or/and the heat-resistant agent is more than one of zirconium phosphate, magnesium phosphate, calcium stearate, magnesium stearate and barium stearate.
Example 11: in the optimization of the embodiment, the plasticizer is more than one of phthalate, terephthalate and acetyl tributyl citrate; or/and the inorganic filler is more than one of calcium carbonate, talcum powder, montmorillonite, mica and magnesium salt whisker.
Example 12: the PBS degradable packaging material with excellent toughness and temperature resistance is prepared by the following method: firstly, uniformly mixing 49 parts of PBS, 14 parts of PBST, 10 parts of PBAT, 3 parts of n-butyl titanate, 1 part of silicon dioxide, 1 part of zirconium phosphate, 2 parts of phthalate and 20 parts of inorganic filler (the inorganic filler is formed by mixing 19 parts of calcium carbonate and 1 part of talcum powder) to obtain a primary mixture; secondly, granulating the primary mixture at 80 ℃ by a double-screw extruder to obtain granular mixed resin; and thirdly, blowing the particle mixed resin into a film with smooth and non-frosted surface by using a double-screw film blowing machine under the conditions that the temperature is 130 ℃ and the rotating speed is 200r/min, thus obtaining the PBS degradable packaging material with excellent toughness and temperature resistance. The double-screw extruder and the double-screw film blowing machine are all the prior known and common equipment.
Example 13: the PBS degradable packaging material with excellent toughness and temperature resistance is prepared by the following method: firstly, uniformly mixing 50 parts of PBS, 12 parts of PBST, 17 parts of PBAT, 3 parts of succinic acid, 0.5 part of silicon dioxide, 1 part of calcium stearate, 1.5 parts of terephthalate and 15 parts of inorganic filler (the inorganic filler is formed by mixing 14 parts of calcium carbonate and 1 part of talcum powder) to obtain a primary mixture; secondly, granulating the primary mixture at 120 ℃ by a double-screw extruder to obtain granular mixed resin; and thirdly, blowing the particle mixed resin into a film with smooth and non-frosted surface by using a double-screw film blowing machine under the conditions that the temperature is 150 ℃ and the rotating speed is 350r/min, thus obtaining the PBS degradable packaging material with excellent toughness and temperature resistance.
Example 14: the PBS degradable packaging material with excellent toughness and temperature resistance is prepared by the following method: step one, uniformly mixing 55 parts of PBS, 10 parts of PBST, 14 parts of PBAT, 5 parts of sebacic acid, 0.8 part of silicon dioxide, 1.3 parts of magnesium stearate, 2.8 parts of acetyl tributyl citrate and 10 parts of inorganic filler (the inorganic filler is formed by mixing 9 parts of calcium carbonate and 1 part of talcum powder) to obtain a primary mixture; secondly, granulating the primary mixture at 188 ℃ through a double-screw extruder to obtain granular mixed resin; and thirdly, blowing the particle mixed resin into a film with smooth and non-frosted surface by using a double-screw film blowing machine under the conditions that the temperature is 145 ℃ and the rotating speed is 280r/min, thus obtaining the PBS degradable packaging material with excellent toughness and temperature resistance.
Example 15: the PBS degradable packaging material with excellent toughness and temperature resistance is prepared by the following method: firstly, uniformly mixing 65 parts of PBS, 37 parts of PBST, 30 parts of PBAT, 6.5 parts of MDI, 0.7 part of silicon dioxide, 0.8 part of barium stearate, 1.9 parts of phthalate and 13 parts of inorganic filler (the inorganic filler is formed by mixing 12 parts of calcium carbonate and 1 part of talcum powder) to obtain a primary mixture; secondly, granulating the primary mixture at 90 ℃ by a double-screw extruder to obtain granular mixed resin; and thirdly, blowing the particle mixed resin into a film with smooth and non-frosted surface by using a double-screw film blowing machine under the conditions that the temperature is 190 ℃ and the rotating speed is 240r/min, thus obtaining the PBS degradable packaging material with excellent toughness and temperature resistance.
PBS (Poly Butylene succinate) degradable packaging materials with excellent toughness and temperature resistance prepared according to the examples 12 to 15 are respectively detected by GB/T1040.2-2006, the elongation at break of the PBS degradable packaging materials with excellent toughness and temperature resistance prepared in the examples 12 to 15 and the existing PLA product films (polylactic acid) is detected, the heat distortion temperature of the PBS degradable packaging materials with excellent toughness and temperature resistance prepared in the examples 12 to 15 and the existing PLA product films is detected by GB/T1633-2000, and the detection results are shown in Table 1. From table 1, under the condition of adding the compatilizer, the inorganic filling is added into the PBS, the PBST and the PBAT, so that the elongation at break and the thermal deformation temperature of the prepared film-shaped PBS degradable packaging material with excellent toughness and temperature resistance are greatly improved, and meanwhile, due to the addition of the compatilizer, the compatibility of the inorganic filling of the rigid nanoparticles with the PBS, the PBST and the PBAT is greatly improved, and the mechanical property of the PBS degradable packaging material with excellent toughness and temperature resistance is improved. Compared with the existing PLA product film, the film material obtained by the component proportion outside the scope of the invention has the physical property far lower than that of the PBS degradable packaging material with excellent toughness and temperature resistance prepared by the invention, so that the prepared PBS film has wider application range and is more practical.
In conclusion, the product prepared by using the PBS with low price has excellent toughness and temperature resistance, can be completely biodegraded, is a good substitute for the existing non-degradable packaging bag, and has the advantages of simple preparation method, easy implementation of production process, environmental protection and saving.
The technical characteristics form an embodiment of the invention, which has strong adaptability and implementation effect, and unnecessary technical characteristics can be increased or decreased according to actual needs to meet the requirements of different situations.
Claims (10)
1. The PBS degradation packaging material with excellent toughness and temperature resistance is characterized by comprising 30 to 70 parts of PBS, 10 to 40 parts of PBST, 10 to 30 parts of PBAT, 2 to 7 parts of compatilizer, 0.3 to 1.5 parts of nucleating agent, 0.3 to 1.5 parts of heat-resistant agent, 1 to 3 parts of plasticizer and 1 to 30 parts of inorganic filler by weight, and is prepared by the following method: firstly, uniformly mixing required amounts of PBS, PBST, PBAT, compatilizer, nucleating agent, heat-resistant agent, plasticizer and inorganic filler to obtain a primary mixture; secondly, granulating the primary mixture at 75-190 ℃ to obtain granular mixed resin; and thirdly, blowing the particle mixed resin into a film with smooth and non-frosted surface under the conditions of 130-190 ℃ and 200-360 r/min of rotation speed to obtain the PBS degradable packaging material with excellent toughness and temperature resistance.
2. The PBS degradation packaging material with excellent toughness and temperature resistance as claimed in claim 1, wherein the raw materials comprise 55 to 60 parts by weight of PBS, 10 to 14 parts by weight of PBST, 10 to 14 parts by weight of PBAT, 3 parts by weight of compatilizer, 0.5 to 1 part by weight of nucleating agent, 1 part by weight of heat-resistant agent, 1 to 2 parts by weight of plasticizer and 10 to 20 parts by weight of inorganic filler.
3. The PBS degradation packaging material with excellent toughness and temperature resistance as claimed in claim 1 or 2, wherein the compatibilizer is one or more of n-butyl titanate, tetrahexyl titanate, succinic acid, sebacic acid, basf ADR4370, MDI, TDI, dicumyl peroxide.
4. The PBS degradation packaging material with excellent toughness and temperature resistance of claim 1, 2 or 3, wherein the nucleating agent is silica, and the mesh number of the silica is 3000 to 5000 mesh.
5. The PBS degradation packaging material with excellent toughness and temperature resistance as claimed in claim 1, 2, 3 or 4, wherein the heat-resistant agent is one or more of zirconium phosphate, magnesium phosphate, calcium stearate, magnesium stearate, barium stearate.
6. The PBS degradation packaging material with excellent toughness and temperature resistance according to any one of claims 1 to 5, wherein the plasticizer is one or more of phthalate, terephthalate and acetyl tributyl citrate.
7. The PBS degradation packaging material with excellent toughness and temperature resistance as claimed in any one of claims 1 to 6, wherein the inorganic filler is at least one of calcium carbonate, talc, montmorillonite, mica, and magnesium salt whisker.
8. A method for preparing the PBS degradable packaging material with excellent toughness and temperature resistance according to any one of claims 1 to 7, which is characterized by comprising the following steps: firstly, uniformly mixing required amounts of PBS, PBST, PBAT, compatilizer, nucleating agent, heat-resistant agent, plasticizer and inorganic filler to obtain a primary mixture; secondly, granulating the primary mixture at 75-190 ℃ to obtain granular mixed resin; and thirdly, blowing the particle mixed resin into a film with smooth and non-frosted surface under the conditions of 130-190 ℃ and 200-360 r/min of rotation speed to obtain the PBS degradable packaging material with excellent toughness and temperature resistance.
9. The method for preparing the PBS degradable packaging material with excellent toughness and temperature resistance as claimed in claim 8, wherein the compatilizer is more than one of n-butyl titanate, tetrahexyl titanate, succinic acid, sebacic acid, basf ADR4370, MDI, TDI, dicumyl peroxide; or/and the nucleating agent is silicon dioxide, and the mesh number of the silicon dioxide is 3000-5000 meshes; or/and the heat-resistant agent is more than one of zirconium phosphate, magnesium phosphate, calcium stearate, magnesium stearate and barium stearate.
10. The method for preparing the PBS degradable packaging material with excellent toughness and temperature resistance as claimed in claim 8 or 9, wherein the plasticizer is one or more of phthalate, terephthalate and acetyl tributyl citrate; or/and the inorganic filler is more than one of calcium carbonate, talcum powder, montmorillonite, mica and magnesium salt whisker.
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| CN115160742A (en) * | 2022-07-12 | 2022-10-11 | 广东春夏新材料科技股份有限公司 | PBAT composite material and preparation method thereof |
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| CN110498939A (en) * | 2019-09-24 | 2019-11-26 | 北京百奥新材科技有限公司 | Long chain branching type Biodegradable polyester composition and preparation method thereof |
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| CN115160742A (en) * | 2022-07-12 | 2022-10-11 | 广东春夏新材料科技股份有限公司 | PBAT composite material and preparation method thereof |
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